CN106521203A - Preparation method of AgCuTi alloy, preparation method of foil strip brazing filler of AgCuTi alloy, and products of AgCuTi alloy - Google Patents
Preparation method of AgCuTi alloy, preparation method of foil strip brazing filler of AgCuTi alloy, and products of AgCuTi alloy Download PDFInfo
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- CN106521203A CN106521203A CN201610998986.5A CN201610998986A CN106521203A CN 106521203 A CN106521203 A CN 106521203A CN 201610998986 A CN201610998986 A CN 201610998986A CN 106521203 A CN106521203 A CN 106521203A
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- 229910017693 AgCuTi Inorganic materials 0.000 title claims abstract description 75
- 239000000956 alloy Substances 0.000 title claims abstract description 64
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000011888 foil Substances 0.000 title claims abstract description 30
- 238000005219 brazing Methods 0.000 title abstract description 7
- 239000000945 filler Substances 0.000 title abstract description 6
- 239000010936 titanium Substances 0.000 claims abstract description 31
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000005097 cold rolling Methods 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims description 29
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 28
- 229910000679 solder Inorganic materials 0.000 claims description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 23
- 239000011812 mixed powder Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 11
- 238000005056 compaction Methods 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 239000012467 final product Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 238000005554 pickling Methods 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 4
- 238000007872 degassing Methods 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 2
- 238000012805 post-processing Methods 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims description 2
- 238000000462 isostatic pressing Methods 0.000 claims 2
- 229910052709 silver Inorganic materials 0.000 abstract description 26
- 239000010949 copper Substances 0.000 abstract description 10
- 229910052802 copper Inorganic materials 0.000 abstract description 9
- 239000000843 powder Substances 0.000 abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 abstract description 8
- 239000001301 oxygen Substances 0.000 abstract description 8
- 238000005204 segregation Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 229910017945 Cu—Ti Inorganic materials 0.000 abstract description 3
- 238000005275 alloying Methods 0.000 abstract description 3
- 238000007789 sealing Methods 0.000 abstract description 3
- 238000005096 rolling process Methods 0.000 abstract description 2
- AHGIVYNZKJCSBA-UHFFFAOYSA-N [Ti].[Ag].[Cu] Chemical compound [Ti].[Ag].[Cu] AHGIVYNZKJCSBA-UHFFFAOYSA-N 0.000 abstract 1
- 239000004332 silver Substances 0.000 description 22
- IUYOGGFTLHZHEG-UHFFFAOYSA-N copper titanium Chemical compound [Ti].[Cu] IUYOGGFTLHZHEG-UHFFFAOYSA-N 0.000 description 18
- 239000000919 ceramic Substances 0.000 description 10
- 229910001069 Ti alloy Inorganic materials 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000005304 joining Methods 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000005476 soldering Methods 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 229910001080 W alloy Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910052774 Proactinium Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000009703 powder rolling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0466—Alloys based on noble metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0425—Copper-based alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
- C22C5/08—Alloys based on silver with copper as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of an AgCuTi alloy, a preparation method of a foil strip brazing filler of the AgCuTi alloy, and products of the AgCuTi alloy. The preparation method is used for solving problems in the prior art that segregation of conventional AgCuTi alloy is easily caused, element Ti is combined with oxygen, activity reducing of brazing filler may be caused in sealing, and in full alloying process, microdefects such as easily caused increasing of grain size and holes are difficult to eliminate, Ag-Ti and Cu-Ti brittle phases are formed from Ti element, and Ag and Cu, and high quality foil strips are difficult to form via rolling. According to the preparation method, vacuum presintering of a powder billet at low temperature is carried out, segregation is inhibited, and hot isostatic pressure medium temperature sintering is adopted, so that grain size and oxygen content are controlled effectively, high density alloy with excellent mechanical properties is obtained, and finally foil strip brazing filler is formed via a plurality of times of direct cold rolling. The preparation method is capable of satisfying requirements on high performance silver copper titanium foil strip brazing filler used in dissimilar material component sealing, is promising in application prospect, and is worthy of large scale popularization and application.
Description
Technical field
The present invention relates to Material Field, especially field of alloy material, specially a kind of preparation method of AgCuTi alloys,
Preparation method of its foil solder and products thereof.
Background technology
Silver-bearing copper brazing filler metal has strength of welded joint height, excellent electric conductivity and corrosion resistance, middle temperature fusing point and good profit
It is moist so as to energy all black and non-ferrous metal of the soldering in addition to aluminium, magnesium and other low-melting-point metals, with relatively broad
Using.Wherein, AgCuTi solder alloys have less angle of wetting, best to the wellability of ceramics, without the need for enter in ceramic surface
The complex metallization pretreatment of row, can realize ceramics with ceramics, ceramics and the disposable soldering success of metal assembly.Thus,
AgCuTi solder alloys obtain many experiments Journal of Sex Research, have important practical significance in fields such as electronics industries.
At present, AgCuTi Alloy Foils band solder preparation technology mainly includes:Vacuum melting, powder rolling shaping and powder smelting
The methods such as gold.Due to AgCuTi alloy constituent element physical differences, in alloy preparation and foil solder forming process, there is following difficulty
Point:1)Three constituent element density variations are larger, and the saturated vapor pressure of component A g is higher(When 685 DEG C ~ 752 DEG C, correspondence saturated vapor pressure
For 10-4 Pa~ 10-3Pa), the easy segregation of solder alloy;2)Element ti activity is larger, under uniform temperature and partial pressure of oxygen, easily and oxygen
With reference to, may cause solder in sealing-in activity reduce;3)In abundant alloying process, crystallite dimension is easily grown up, hole etc.
The more difficult elimination of microdefect, and Ti elements can form Ag-Ti, Cu-Ti brittlement phase with Ag, Cu, it is more difficult to roll forming high-quality paper tinsel
Band.This limits use of the high-quality AgCuTi foil solder under some special applications backgrounds all to a certain extent.
For this purpose, in the urgent need to a kind of new method, to solve the above problems.
The content of the invention
The present invention goal of the invention be:For the easy segregation of existing AgCuTi solder alloys, element ti therein easily with
Oxygen is combined, and solder activity in sealing-in may be caused to reduce, and in abundant alloying process, crystallite dimension is easily grown up, hole
Etc. the more difficult elimination of microdefect, and Ti elements can form Ag-Ti, Cu-Ti brittlement phase with Ag, Cu, it is more difficult to roll forming high-quality
The problem of foil, there is provided a kind of preparation method of AgCuTi alloys, preparation method of its foil solder and products thereof.The present invention is logical
Cross to powder base that vacuum is pre-sintered at low temperature, suppress segregation, with reference to high temperature insostatic pressing (HIP) intermediate sintering temperature, can effective control crystallite dimension and
Oxygen content, obtains the high dense alloy of excellent in mechanical performance, can finally pass through the cold rolling direct forming foil solder of multi-pass.This
It is bright to meet foreign material component sealing-in demand of the high-performance silver-bearing copper titanium foil with solder in microwave change system, with preferable
Application prospect, is worth large-scale promotion and application.
To achieve these goals, the present invention is adopted the following technical scheme that:
A kind of preparation method of AgCuTi alloys, comprises the steps:
(1)Prepare AgCuTi mixed powder for alloy
Silver powder, copper powder, titanium valve are weighed respectively by AgCuTi alloys design requirement, and the silver powder, copper powder, the mass ratio of titanium valve are
25-75:25-75:1-6, obtains the first mixture, loads ball grinder after the first mixture is mixed with titanium abrading-ball, abrasive media
In, wet ball grinding is carried out, the slurry after wet ball grinding Jing after precipitating, be dried, obtains AgCuTi mixed-powders successively;
(2)Mixed powder shaping
By step(1)After the AgCuTi mixed-powders of preparation load mantle, cold isostatic compaction is carried out, base of colding pressing is obtained;
(3)It is pre-sintered
By step(2)The base of colding pressing for preparing carries out vacuum pre-sintering, obtains AgCuTi sintered bodies;
(4)High temperature insostatic pressing (HIP) is densified
By step(3)The AgCuTi sintered bodies of preparation load jacket, after heated degasification, carry out hip moulding;
(5)Post processing
By step(4)The material of hip moulding, carries out the demoulding, obtains final product AgCuTi alloys.
By step(5)Material after the demoulding cuts into bulk, and pickling removes the oxide-film on bulk surface, realizes to AgCuTi
The process of alloy.
By step(5)Line of material after the demoulding cuts into the bulk that thickness is 1 ~ 5mm.
In the step 1, the particle diameter of titanium abrading-ball is 3 ~ 8mm, and abrasive media is absolute ethyl alcohol.
First mixture, titanium abrading-ball, the mass ratio of abrasive media are(1~2)∶(4~12)∶(1~4).
In the step 1, rotational speed of ball-mill is 120~300r/min, and Ball-milling Time is 2~20h.
In the step 2, the static pressure pressure of cold isostatic compaction is 120MPa~270MPa, time 5min~60min.
In the step 3, by step(2)The base of colding pressing for preparing is less than 5 × 10 in vacuum-3Pa, at 600 DEG C~680 DEG C
Vacuum pre-sintering 30min ~ 180min, so as to get AgCuTi sintered bodies consistency be 75% ~ 85%.
In the step 4, the temperature of hip moulding is 700 DEG C~800 DEG C, and pressure is 80MPa ~ 140MPa, the time
For 5min~90min.
Aforementioned preparation method of the AgCuTi Alloy Foils with solder, comprises the steps:The AgCuTi alloys for obtaining are being rolled
The AgCuTi foil solders that multi-pass is cold rolling, until obtaining 0.08mm~0.12mm are carried out on machine.
Reduction in pass 5% ~ 20%.
Product prepared by aforementioned AgCuTi alloy preparation methods, the consistency of the product is 99.00% ~ 99.99%.
For foregoing problems, the present invention provides a kind of preparation method of AgCuTi alloys, the preparation method of its foil solder
And products thereof.Wherein, be related to Ag, Cu, Ti mixed-powder prepare, shaping, low temperature presintering knot, high temperature insostatic pressing (HIP) intermediate sintering temperature and cold rolling
Etc. step.Wherein, the preparation method of AgCuTi alloys comprises the steps.
In the present invention, first by silver powder, copper powder and titanium valve according to design requirement, proportion ingredient, silver powder, copper powder, titanium are carried out
The mass ratio of powder is 25-75:25-75:1-6, obtains the first mixture, and the first mixture is mixed with titanium abrading-ball, abrasive media
Load in ball grinder afterwards, carry out wet ball grinding, the slurry after wet ball grinding Jing after precipitating, be dried, obtains AgCuTi mixing successively
Powder.Then, after mixed the AgCuTi mixed-powders after proportioning with titanium abrading-ball and abrasive media, load stainless steel jar mill
In;After ball grinder is sealed, being placed on planetary ball mill carries out wet grinding, first with 200 mesh wire-mesh screens by titanium after grinding
Abrading-ball is separated with slip, and subsequent slip obtains AgCuTi mixed-powders Jing after precipitating, be dried.
Further, abrading-ball particle diameter is the titanium ball of 3~8mm, and abrasive media is absolute ethyl alcohol.Preferably, AgCuTi alloys
Powder, abrading-ball and absolute ethyl alcohol according to mass ratio are(1~2)∶(4~12)∶(1~4)Ratio mixing.Drum's speed of rotation is
120~300r/min, milling time are 2~20h.
Then, then by the AgCuTi mixed-powders obtained after grinding load in soft mode, carry out cold isostatic compaction, be obtained cold
Pressed compact.Base of colding pressing again carries out vacuum pre-sintering, obtains AgCuTi sintered bodies.AgCuTi sintered bodies sample is being loaded into stainless steel
After jacket heating degasification, high temperature insostatic pressing (HIP) intermediate sintering temperature is carried out.The material of hip moulding is carried out, after the demoulding, obtaining final product AgCuTi
Alloy.
Further, cold isostatic compaction pressure is 120~270MPa, 5~60min of time;By the blank after isostatic cool pressing
Carry out vacuum-sintering, sintering temperature:600 DEG C~680 DEG C, vacuum is less than 5 × 10-3Pa, temperature retention time:30min ~ 180min,
After sintering, the consistency of sample is 75% ~ 85%;Hip temperature is 700 DEG C~800 DEG C, and pressure is 80MPa ~ 140MPa, is protected
The pressure time is 5~90min.
The AgCuTi alloys that material after high temperature insostatic pressing (HIP) intermediate sintering temperature is obtained Jing after the demoulding, then warp cut into thickness for 1 ~
The bulk of 5mm, removes surface film oxide with pickling.Finally, the AgCuTi alloys for obtaining are carried out into multi- pass rolling on cold-rolling mill,
AgCuTi foil solders until obtaining 0.08mm~0.12mm.
Fig. 1,2 sets forth the AgCuTi foil solder figures of present invention preparation, AgCuTi alloys micro-organization chart.Jing is surveyed
Fixed, using the consistency of the AgCuTi alloys prepared by the present invention up to 99% ~ 99.99%, and composition is uniform, crystallite dimension is thin
Little, oxygen content is less than 800ppm, and to ceramic/metal, metal/metal material has good sealing property.
Energy effective control AgCuTi alloy brittlement phase type and quantity of the invention, the alloy of preparation have good mechanical property
Can, consistency is 99% ~ 99.99%.Meanwhile, the present invention in, alloy by multi-pass it is cold rolling can direct forming foil solder, work
Skill is simple.AgCuTi foil solders composition prepared by the present invention is uniform, and crystal grain is tiny, and oxygen content is low, and size is controllable, can expire
The sealing-in demand of key component in sufficient microwave change system.Jing actual tests, the present invention can meet key in microwave change system
The demand of component sealing-in, has been successfully applied to Al2O3Ceramics/4J33 alloys, tungsten/steel, the sealing-in of graphite/Cu.
Description of the drawings
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein:
Fig. 1 is the AgCuTi foil solder figures prepared by the present invention.
Fig. 2 is the AgCuTi alloys micro-organization chart prepared by the present invention.
During Fig. 3 is embodiment 1,4J33 alloys and Al2O3Ceramic joining interface micro-organization chart.
During Fig. 4 is embodiment 2, copper alloy and joining of graphite figure.
During Fig. 5 is embodiment 3, tungsten alloy and G50 steel linkage interfaces micro-organization chart.
Specific embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive
Feature and/or step beyond, can combine by any way.
Any feature disclosed in this specification, unless specifically stated otherwise, can be equivalent or with similar purpose by other
Alternative features are replaced.I.e., unless specifically stated otherwise, each feature is an example in a series of equivalent or similar characteristics
.
Embodiment 1
1)By silver, copper, titanium simple substance powder according to percentage by weight 69.5:27.5:3 carry out dispensing, obtain the first mixture.By first
Mixture is put into after being mixed by 1: 6: 1 mass ratio with titanium abrading-ball, absolute ethyl alcohol in stainless steel jar mill carries out ball milling;Wherein, grind
Spherolite footpath is 3mm.After by ball grinder good seal, insert, batch can rotating speed is 100r/
Min, time are 2h;After grinding, first titanium abrading-ball is separated with slip with 200 mesh wire-mesh screens, slip is obtained Jing after precipitating, be dried
To silver-bearing copper titanium mixed-powder.
2)The silver-bearing copper titanium mixed-powder obtained after grinding is loaded after soft mode, using cold isostatic compaction, pressure is
120MPa, time 5min, are obtained base of colding pressing.
3)Base of colding pressing after by isostatic cool pressing carries out vacuum-sintering, sintering temperature:600 DEG C, temperature retention time:30min, sintering
The consistency of sample is 75% afterwards, obtains final product AgCuTi sintered bodies.
4)AgCuTi sintered bodies sample after pre-sintering is carried out into high temperature insostatic pressing (HIP) intermediate sintering temperature, hip temperature is 700
DEG C, the dwell time is 30min, pressure 80MPa.
5)Material Jing after high temperature insostatic pressing (HIP) Jing after the demoulding, the silver-bearing copper titanium alloy for obtaining.The silver-bearing copper titanium alloy line for obtaining is cut
The bulk that thickness is 1 ~ 5mm is cut into, then surface film oxide is removed with pickling.The consistency of the alloy is 99.9%, tensile strength
270MPa, elongation percentage 22%.
6)It is cold rolling that silver-bearing copper titanium bulk alloy to preparing carries out multi-pass, reduction in pass 10%, and direct forming thickness is
The foil of 0.12mm.
7)To prepared silver-bearing copper titanium foil band solder pressure process soldering 4J33 alloys and Al2O3Ceramics, shearing strength of joint
98MPa。
Fig. 3 is given in the present embodiment, 4J33 alloys and Al2O3Ceramic joining interface micro-organization chart.
Embodiment 2
1)By silver, copper, titanium simple substance powder according to percentage by weight 30.5:65.5:4 carry out dispensing dispensing, obtain the first mixture.Will
First mixture is put into after being mixed by 2: 8: 2 mass ratioes with titanium abrading-ball, absolute ethyl alcohol in stainless steel jar mill carries out ball milling;Its
In, abrading-ball particle diameter is 5mm.After by ball grinder good seal, insert, batch can rotating speed is
200r/min, time are 8h;After grinding, first titanium abrading-ball is separated with slip with 200 mesh wire-mesh screens, slip Jing is precipitated, is dried
Afterwards, obtain silver-bearing copper titanium mixed-powder.
2)The silver-bearing copper titanium alloy mixed-powder obtained after grinding is loaded after soft mode, using cold isostatic compaction, pressure is
180MPa, time 10min, are obtained base of colding pressing.
3)Base of colding pressing after by isostatic cool pressing carries out vacuum-sintering, sintering temperature:650 DEG C, temperature retention time:120min, burns
After knot, the consistency of sample is 78%, obtains final product AgCuTi sintered bodies.
4)AgCuTi sintered bodies after vacuum-sintering are carried out into high temperature insostatic pressing (HIP) intermediate sintering temperature, hip temperature is 750 DEG C,
Dwell time is 60min, pressure 120MPa.
5)The silver-bearing copper titanium alloy that material Jing after high temperature insostatic pressing (HIP) is obtained Jing after the demoulding.By the silver-bearing copper titanium alloy wire cutting for obtaining
Into the bulk that thickness is 1 ~ 5mm, then surface film oxide is removed with pickling.The consistency of the alloy is 99.9%, tensile strength
350MPa, elongation percentage 20%.
6)It is cold rolling that silver-bearing copper titanium bulk alloy to preparing carries out multi-pass, reduction in pass 5%, and direct forming thickness is
The foil of 0.1mm.
7)To prepared silver-bearing copper titanium foil band solder pressure process copper brazing alloy and graphite, shearing strength of joint 16.5MPa.
During Fig. 4 is embodiment 2, copper alloy and joining of graphite figure.
Embodiment 3
1)By silver, copper, titanium simple substance powder according to percentage by weight 70.5:26:3.5 carry out dispensing, obtain the first mixture.By first
Mixture is put into after being mixed by 2: 10: 4 mass ratioes with titanium abrading-ball, absolute ethyl alcohol in stainless steel jar mill carries out ball milling;Wherein, grind
Spherolite footpath is 8mm.After by ball grinder good seal, insert, batch can rotating speed is 300r/
Min, time are 10h;After grinding, first titanium abrading-ball is separated with slip with 200 mesh wire-mesh screens, slip is obtained Jing after precipitating, be dried
To silver-bearing copper titanium mixed-powder.
2)After the titanium alloy mixed-powder obtained after step one is ground loads soft mode, using cold isostatic compaction, pressure
For 270MPa, time 60min, base of colding pressing is obtained.
3)Base of colding pressing after by isostatic cool pressing carries out vacuum pre-sintering, sintering temperature:680 DEG C, temperature retention time:180min,
After sintering, the consistency of sample is 85%, obtains final product AgCuTi sintered bodies.
4)AgCuTi sintered bodies after vacuum-sintering are carried out into high temperature insostatic pressing (HIP) intermediate sintering temperature, hip temperature is 800 DEG C,
Dwell time is 60min, pressure 140MPa
5)Material Jing after high temperature insostatic pressing (HIP) Jing after the demoulding, the silver-bearing copper titanium alloy for obtaining.By the silver-bearing copper titanium alloy wire cutting for obtaining into
Bulk of the thickness for 1 ~ 5mm, then surface film oxide is removed with pickling.The consistency of the alloy is 99.99%, and intensity 285MPa extends
Rate 21.5%.
6)It is cold rolling that silver-bearing copper titanium bulk alloy to preparing carries out multi-pass, reduction in pass 20%, and direct forming thickness is
The foil of 0.08mm.
7)To prepared silver-bearing copper titanium foil band solder pressure process soldering tungsten alloy and G50 steel, joint tensile strength 430MPa.
Fig. 5 is given in the present embodiment, tungsten alloy and G50 steel linkage interfaces micro-organization chart.
The invention is not limited in aforesaid specific embodiment.The present invention is expanded to and any is disclosed in this manual
New feature or any new combination, and the arbitrary new method that discloses or the step of process or any new combination.
Claims (9)
1. a kind of preparation method of AgCuTi alloys, it is characterised in that comprise the steps:
(1)Prepare AgCuTi mixed powder for alloy
Silver powder, copper powder, titanium valve are weighed respectively by AgCuTi alloys design requirement, and the silver powder, copper powder, the mass ratio of titanium valve are
25-75:25-75:1-6, obtains the first mixture, loads ball grinder after the first mixture is mixed with titanium abrading-ball, abrasive media
In, wet ball grinding is carried out, the slurry after wet ball grinding Jing after precipitating, be dried, obtains AgCuTi mixed-powders successively;
(2)Mixed powder shaping
By step(1)After the AgCuTi mixed-powders of preparation load mantle, cold isostatic compaction is carried out, base of colding pressing is obtained;
(3)It is pre-sintered
By step(2)The base of colding pressing for preparing carries out vacuum pre-sintering, obtains AgCuTi sintered bodies;
(4)High temperature insostatic pressing (HIP) is densified
By step(3)The AgCuTi sintered bodies of preparation load jacket, after heated degasification, carry out hip moulding;
(5)Post processing
By step(4)The material of hip moulding, carries out the demoulding, obtains final product AgCuTi alloys.
2. the preparation method of AgCuTi alloys according to claim 1, it is characterised in that by step(5)Material after the demoulding
Bulk is cut into, pickling removes the oxide-film on bulk surface, realizes the process to AgCuTi alloys.
3. the preparation method of AgCuTi alloys according to claim 1, it is characterised in that in the step 1, rotational speed of ball-mill is
120~300r/min, Ball-milling Time are 2~20h.
4. according to any one of claim 1-3 AgCuTi alloys preparation method, it is characterised in that it is in the step 2, cold
The static pressure pressure of isostatic pressing is 120MPa~270MPa, time 5min~60min.
5. according to any one of claim 1-4 AgCuTi alloys preparation method, it is characterised in that in the step 3, will
Step(2)The base of colding pressing for preparing is less than 5 × 10 in vacuum-3Pa, vacuum pre-sintering 30min ~ 180min at 600 DEG C~680 DEG C,
The consistency for making the AgCuTi sintered bodies for obtaining is 75% ~ 85%.
6. according to any one of claim 1-5 AgCuTi alloys preparation method, it is characterised in that in the step 4, heat
The temperature of isostatic pressing is 700 DEG C~800 DEG C, and pressure is 80MPa ~ 140MPa, and the time is 5min~90min.
7. the foil solder preparation method of AgCuTi alloys described in aforementioned any one of claim 1-6, comprises the steps:Will
To AgCuTi alloys carry out that multi-pass is cold rolling on milling train, the AgCuTi foil solders until obtaining 0.08mm~0.12mm.
8. preparation method according to claim 7, it is characterised in that reduction in pass 5% ~ 20%.
9. the product described in aforementioned any one of claim 1-5 prepared by AgCuTi alloy preparation methods, the consistency of the product
For 99.00% ~ 99.99%.
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Cited By (7)
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CN109622938A (en) * | 2018-12-12 | 2019-04-16 | 江苏阳明船舶装备制造技术有限公司 | It is a kind of to prepare copper alloy surface wear-resistant coating and preparation method with AgCuTi |
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2009235477A (en) * | 2008-03-27 | 2009-10-15 | Furukawa-Sky Aluminum Corp | Aluminum alloy sheet for drink can barrel, and method for producing the same |
CN105537799A (en) * | 2015-12-24 | 2016-05-04 | 昆明贵金属研究所 | Agcuti active brazing filler metal and preparation method thereof |
-
2016
- 2016-11-14 CN CN201610998986.5A patent/CN106521203B/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2009235477A (en) * | 2008-03-27 | 2009-10-15 | Furukawa-Sky Aluminum Corp | Aluminum alloy sheet for drink can barrel, and method for producing the same |
CN105537799A (en) * | 2015-12-24 | 2016-05-04 | 昆明贵金属研究所 | Agcuti active brazing filler metal and preparation method thereof |
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CN109971995A (en) * | 2019-04-02 | 2019-07-05 | 东北大学 | A kind of high crisp copper-titanium alloy and preparation method thereof firmly |
CN109971987A (en) * | 2019-04-02 | 2019-07-05 | 东北大学 | A kind of grinding wheel base body copper-titanium alloy and preparation method thereof |
CN109971988A (en) * | 2019-04-02 | 2019-07-05 | 东北大学 | A kind of superhigh intensity copper-titanium alloy and preparation method thereof |
CN111519079A (en) * | 2020-04-15 | 2020-08-11 | 燕山大学 | CoCrNiCuFeMnAl high-entropy alloy and preparation method thereof |
CN111519079B (en) * | 2020-04-15 | 2021-09-10 | 燕山大学 | CoCrNiCuFeMnAl high-entropy alloy and preparation method thereof |
CN114951873A (en) * | 2022-06-14 | 2022-08-30 | 浙江亚通焊材有限公司 | Composite solder containing high-entropy alloy and method for connecting AlN and Cu through brazing |
CN114951873B (en) * | 2022-06-14 | 2023-10-03 | 浙江亚通新材料股份有限公司 | Composite brazing filler metal containing high-entropy alloy and method for brazing and connecting AlN and Cu by composite brazing filler metal |
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